WO2011143792A1 - 可剥离型光转换发光膜 - Google Patents

可剥离型光转换发光膜 Download PDF

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Publication number
WO2011143792A1
WO2011143792A1 PCT/CN2010/000716 CN2010000716W WO2011143792A1 WO 2011143792 A1 WO2011143792 A1 WO 2011143792A1 CN 2010000716 W CN2010000716 W CN 2010000716W WO 2011143792 A1 WO2011143792 A1 WO 2011143792A1
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WO
WIPO (PCT)
Prior art keywords
light
fluorescent material
film
agent
converting
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PCT/CN2010/000716
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English (en)
French (fr)
Inventor
肖志国
李茂龙
常英
隋玉龙
戴兴建
吴粤宁
张宏伟
Original Assignee
大连路明发光科技股份有限公司
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Application filed by 大连路明发光科技股份有限公司 filed Critical 大连路明发光科技股份有限公司
Priority to EP10851551.1A priority Critical patent/EP2572878A4/en
Priority to CN201080066635.1A priority patent/CN102869502B/zh
Priority to KR1020127033204A priority patent/KR20130083388A/ko
Priority to JP2013510466A priority patent/JP2013534713A/ja
Priority to PCT/CN2010/000716 priority patent/WO2011143792A1/zh
Priority to US13/699,136 priority patent/US20130089729A1/en
Publication of WO2011143792A1 publication Critical patent/WO2011143792A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils

Definitions

  • the invention belongs to the field of LED display and illumination technology.
  • the invention relates to a strippable fluorescent material light-converting luminescent film, which can convert blue light emitted by an LED into white light, and specifically relates to a layered film product made of a luminescent material, a luminescent coating and a resin film. It also relates to a peelable light-converting luminescent film for a light-emitting device including an LED backlight, a digital display, and illumination. Background technique
  • the current LED backlights, digital display and illumination devices are usually obtained by encapsulating fluorescent materials.
  • the white light emitting device prepared by the method is difficult to ensure the consistency of brightness, color coordinates, color temperature and color rendering, and since the phosphor is close to the chip, it is easily affected by heat and the life is lowered.
  • WO2007049187 describes a sealing film agent for silicone-doped phosphor, which is mounted on a blue LED to achieve the purpose of converting blue light into white light, but the material itself is a film-like structure, which needs to be used according to the use. Laminated party Secondary molding, complex process.
  • U.S. Patent No. 6,600,175 B1 mentions the use of organic fluorescent and phosphorescent materials in a white LED package for packaging instead of LED phosphors. The composite emits white light, which is only a single device coating, and can only be realized simply by using an electric light source. Certain difficulty.
  • Patent CN1 01 533882A introduces a phosphor pre-formed film for white LED and a preparation method thereof, which is prepared by screen printing method, and the continuous and large-area film production cannot be realized in the process.
  • Patent CN1 01443192A discloses a photoluminescent plate.
  • the photoluminescent plate In order to protect the matrix resin layer and improve heat resistance and moisture resistance, the photoluminescent plate preferably uses a PET polyester film as a protective film, although after removing the protective film, The photoluminescent plate is used, but it is generally preferred to maintain a protective film for adhesion for protection.
  • the photoluminescence plate is prepared by screen printing, slit coating or roll coating, etc., by printing a mixture of a phosphor or the like and adjusting the viscosity of the silicone resin mixture onto the protective film.
  • the board usually has a thin luminescent coating and is difficult to produce a thicker luminescent coating.
  • An object of the present invention is to provide a peelable type light-converting film which is used as a substrate and a protective film by a fluorine-based polyester film which can be easily peeled off when used in a light-converting film.
  • the prepared peelable light conversion film has high uniformity, good homogenization, anti-glare, high light conversion efficiency, low cost, excellent aging performance, and simple production process.
  • the peelable type light-converting luminescent film according to the present invention is composed of a substrate and a photo-conversion coating layer thereon, and the photo-transformation coating layer is composed of a fluorescent material, a two-component silicone resin, a diluent, and an auxiliary agent.
  • the substrate described above is a fluorocarbon polyester film which is used as a substrate when preparing a light-converting luminescent film to function as a protective film; it can be easily peeled off from the photo-converting coating layer during use. Since the fluorine polyester film is used as the substrate, when the light conversion luminescent film is prepared, it can function as a coating production substrate and a protective film. In addition, due to the use of the light conversion coating layer, the main resin is silicone.
  • the resin itself is soft and elastic, and is easily deformed when the protective film is peeled off, resulting in uneven thickness of the light conversion film, thereby affecting the luminescent property. Therefore, the present invention uses a fluorocarbon polyester film as a substrate and a protective film. When used, the light conversion coating layer can be easily peeled off from the fluorine polyester film, thereby avoiding deformation due to stretching, and ensuring that the products of the light conversion film are hooked and stable.
  • the fluoropolyester film is a polyester film coated with a fluorine release agent.
  • the thickness is preferably 20 - ⁇ ⁇ , and the fluorocarbon polyester film is used as a substrate when preparing the light-converting luminescent film, and can be easily peeled off from the photo-transformed coating layer when used, so that the blue light source is directly irradiated to the light-converting luminescence On the film, the refraction of light in the fluorocarbon polyester film is reduced, and the overall luminous efficiency is improved.
  • the fluorescent material is a combination of one or both of an aluminate fluorescent material, a silicate fluorescent material, a silicon nitride fluorescent material, and a sulfur oxide fluorescent material that can be excited by blue light; the fluorescent material is used as an emission of an excitation light source.
  • the aperture is excited by a blue LED in the range of 440 ⁇ 475nm, and absorbs at least one emission spectrum with a peak wavelength in the range of 525 ⁇ 650nm; the light emitted by the fluorescent material is combined with the light emitted by the blue LED to form a white or other color. Light.
  • the fluorescent material used in the invention needs to be treated by a mixture of ethanol-alkoxy oligosiloxane, and the fluorescent material can be treated with the mixed solution to improve the compatibility with the silicone resin and improve the surface state of the coating film. .
  • the treatment of the fluorescent material is a heat treatment method, and the specific steps are at a temperature of 80 to 90.
  • the fluorescent material and ethanol are put into the reaction kettle in proportion, stirred, and then the alkoxy oligosiloxane is put into the reaction vessel, stirred together with the powder, and finally the powder mixture after the treatment is carried out. Filtering and drying, the obtained fluorescent material can be directly used in the preparation of the photo-conversion coating.
  • the silicone resin used in the present invention is a two-component addition-warmed vulcanized liquid silicone resin which is transparent, soft and elastic. This resin has good thermal oxidation stability, excellent electrical insulation properties, excellent moisture resistance, water resistance, rust resistance, cold resistance and resistance. Ozone and weather resistance. The resin does not yellow when it is operated at a high temperature for a long time, and is still flexible and has high strength after curing.
  • the silicone resin to be used in the present invention is preferably a silicone resin having a viscosity of from 3,000 to 5,000 cp.s and a light transmittance of >85%.
  • the preparation process of the peelable type light-converting luminescent film according to the present invention is as follows: the fluorescent material is first treated by a mixture of ethanol-alkoxy oligosiloxane, and the fluorescent material treated by the mixed solution, two-component organic
  • the silicone resin, the diluent and the auxiliary agent are combined by grinding, dispersing and mixing according to the ratio, and after being filtered and defoamed, coated on the surface of the fluorine polyester film, and solidified to obtain a finished product; the curing is formed into heat curing Forming, curing temperature: 150 ⁇ 200. C.
  • the diluent is one or more of toluene, diphenylbenzene, butyl ester, ethyl ester, mercapto silicone oil, dimercapto silicone oil, ethyl silicone oil, phenyl silicone oil, and methylphenyl silicone oil.
  • the auxiliary agent may be one or more of an ultraviolet light absorber, a stabilizer, a leveling agent, an antifoaming agent, a flame retardant, an anti-settling agent, a wetting agent, and an antistatic agent.
  • the fluorine polyester film in the peelable type light conversion film is used as a substrate at the time of preparation, it can function as a protective film; it can be easily peeled off during use to avoid deformation of the light conversion coating layer, after peeling Reduces the refraction of light and improves luminous efficiency.
  • the compatibility with the silicone resin is improved, the surface state of the coating film is improved, and the surface property is improved. Uniformity of the film.
  • the peelable type light conversion film prepared by the coating method can realize the coating requirements of different thicknesses, and the light conversion film of various thicknesses can be prepared, and continuous production can be realized, and the production efficiency is high.
  • the viscosity of the light conversion coating and the particle size of the fluorescent material are relatively wide by the coating method, it is easier to produce. detailed description
  • Fluorescent material pretreatment The fluorescent material is placed at a temperature of 80 with a ratio of 1:4. The reaction vessel of C was stirred, and then the alkoxy oligosiloxane was put into the reaction vessel according to 3% of the fluorescent material, and stirred with the powder for 20 minutes, and the powder solution after the treatment was suction filtered, dried and treated. The fluorescent material is ready for use.
  • the treated fluorescent material and other raw materials are formulated into a mixture according to the following formula (mass percentage):
  • Fluorescent material pretreatment The fluorescent material and ethanol were put into a reactor at a temperature of 90 ° C in a ratio of 1:3, stirred, and then the methoxy oligosiloxane was irradiated at 4 °/. The mixture was placed in a reaction vessel and stirred with the powder for 30 minutes. The treated powder was suction filtered and dried to obtain a treated fluorescent material for use.
  • the treated fluorescent material and other raw materials are formulated into a mixture by the following formula (% by weight):
  • Fluorescent material pretreatment Put the fluorescent material in a ratio of 1:3 to the temperature of 85. The reaction vessel of C was stirred, and then the alkoxy oligosiloxane was put into the reaction vessel at 2% of the fluorescent material, and stirred with the powder for 20 minutes. The treated powder liquid was suction filtered and dried to obtain a good treatment. The fluorescent material is ready for use.
  • the treated fluorescent material and other raw materials are formulated into a mixed solution by the following formula (mass percentage):
  • the silicon oxide fluorescent material 4. 0 The silicon oxide fluorescent material 4. 0
  • the defoaming agent 0. 2 The dispersing agent 0. 4
  • Silicon nitride fluorescent material 4. 0 The above raw materials are ground, dispersed and mixed, and then filtered, defoamed, coated on the surface of the ⁇ fluorocarbon polyester film, and solidified to obtain a finished product.
  • the curing temperature is 180 ° C, 2 min.
  • Fluorescent material itt pretreatment The fluorescent material is placed at a temperature of 90 with a ratio of 1:3. The reaction vessel of C was stirred, and then the alkoxy oligosiloxane was put into the reaction vessel at 4% of the fluorescent material, and stirred with the powder for 30 minutes. The treated powder liquid was suction filtered, dried and treated. The fluorescent material is ready for use.
  • the treated fluorescent material and other raw materials are formulated into a mixed solution by the following formula (mass percentage):
  • Fluorescent material pretreatment The luminescent material was placed at a temperature of 80 with a ratio of 1:4. The reaction vessel of C was stirred, and then the alkoxy oligosiloxane was put into the reaction kettle as 3% of the luminescent material, and stirred with the powder for 20 minutes, and the powder after the treatment was processed. The body fluid is subjected to suction filtration, and dried to obtain a treated fluorescent material to be used.
  • the treated fluorescent material and other raw materials are formulated into a mixture by the following formula (mass ratio):
  • Fluorescent material pretreatment The fluorescent material and ethanol are put into a reaction kettle at a temperature of 90 ° C in a ratio of 1:3, stirred, and then the alkoxy oligosiloxane is put into the reaction vessel as 4% of the luminescent material, and The powder was stirred for 30 minutes, and the treated powder liquid was subjected to suction filtration, and dried to obtain a treated fluorescent material for use.
  • the treated fluorescent material and other raw materials are formulated into a mixed solution by the following formula (mass percentage):
  • Silicon nitride fluorescent material Water 85. 4 The above raw materials are ground, dispersed and mixed, and then filtered and defoamed, coated on the surface of a 50 ⁇ ⁇ fluorinated polyester film, and solidified to obtain a finished product.
  • the curing temperature is 200 ° C, 2 min.
  • Fluorescent material pretreatment The fluorescent material is placed at a temperature of 90 with a ratio of 1:3. The reaction vessel of C was stirred, and then the alkoxy oligosiloxane was put into the reaction vessel at 4% of the fluorescent material, and stirred with the powder for 30 minutes. The treated powder liquid was suction filtered, dried and treated. The fluorescent material is ready for use.
  • the treated fluorescent material and other raw materials are formulated into a mixed solution by the following formula (mass percentage):
  • Fluorescent material pretreatment The fluorescent material was put into a temperature of 85 at a ratio of 1:3. The reaction vessel of C was stirred, and then the alkoxy oligosiloxane was put into the reaction vessel at 2% of the fluorescent material, and stirred with the powder for 20 minutes, and the treated powder was mixed. The body fluid is subjected to suction filtration, and dried to obtain a treated fluorescent material to be used.
  • the treated fluorescent material and other raw materials are formulated into a mixed solution by the following formula (mass percentage):
  • Aluminate fluorescent material 4. 0 water 87. 7
  • the above raw materials are ground, dispersed and mixed, filtered, defoamed, coated on the surface of ⁇ ⁇ fluorocarbon polyester film, cured to form a finished product, curing temperature For: 180. C, 2min.

Description

可剥离型光转换发光膜
技术领域
本发明属于 LED显示和照明技术领域。涉及可剥离型荧光材 料光转换发光膜， 能够将 LED发出的蓝光转换为白光， 具体涉及 发光材料、 发光涂料和树脂膜制成的层状膜产品。 同时涉及包 括 LED 背光源、 数码显示及照明在内的发光装置用的可剥离型 光转换发光膜。 背景技术
目前的 LED 背光源、 数码显示及照明装置通常是采用封装 荧光材料的方式得到的， 此类专利也已经有很多如中国专利 CN1941431 〈白色发光元件及其制造方法>， CN151 0766 〈表面安 装型白色发光二极管〉， CN1 01 186818 〈蓝紫光或蓝光激发的荧 光体及制造方法与封装的白光二极管 >， 均为荧光材料混合在树 脂中涂覆在 LED 芯片上制成白色发光器件。 该方法制备出的白 光发光器件很难保证亮度、 色坐标、 色温和显色性的一致性， 并且由于荧光粉贴近芯片， 受到热量的影响很容易引起老化， 寿命降低。 国际专利 WO20071 05853介绍了一种光致发光膜的制 备方法， 所釆用的发光材料为无机发光材料， 该专利采用涂膜 方式在基材膜上进行制备， 并未对具体工艺进行介绍， 并且制 备出的光致发光膜与基材结合为一体， 在使用中由于基材物质 折射率与光致发光层并不一致， 会损失部分光效。 国际专利
WO2007049187 介绍了一种釆用硅酮掺杂磷光体的密封膜剂， 将 这种膜材料安装在蓝光 LED 上， 达到蓝光转换为白光的目的， 但是这种材料本身为膜状结构， 需根据使用情况采用层压的方 式二次成型， 工艺复杂。 美国专利 US 6600175B1提及在白光 LED 封装中采用有机荧光、 磷光材料， 替代 LED 荧光粉进行封装， 复合发出白光， 只是单个器件的涂装， 只能简单实现电光源， 在面光源的应用上有一定难度。 中国专利 CN1 01 533882A介绍了 一种白光 LED 用荧光粉预制薄膜及其制备方法， 采用的是丝网 印刷的方法进行制备， 工艺上无法实现连续、 大面积膜的生产。 专利 CN1 01443192A公开了一种光致发光板， 为了保护基质树脂 层， 提高耐热性和耐湿性， 该光致发光板优选采用 PET 聚酯膜 为保护膜， 虽然在移除保护膜之后也可以使用该光致发光板， 但通常是优选保持粘附的保护膜， 用于保护作用。 另外该光致 发光板采用丝网印刷、 狭缝涂覆或辊涂等将加入荧光体等并调 节好粘度的有机硅树脂混合液印刷到保护膜上的方法制备， 这 样制得的光致发光板通常发光涂层较薄， 如果需生产较厚发光 涂层时有难度。
发明内容
本发明的目的是提供一种可剥离型光转换膜， 该膜采用氟 素聚酯膜作为基材和保护膜使用，在光转换膜使用时可以将其很 容易剥离。 制备的可剥离性光转换膜均匀度高、 匀光性好、 防眩 光、 光转换效率高、 成本低、 老化性能优异、 生产工艺简单。
本发明涉及的可剥离型光转换发光膜由基材和在其上的光 转化涂料层构成， 光转化涂料层由荧光材料、 双组分有机硅树 脂、 稀释剂和助剂组成。 其中所述的基材为氟素聚酯膜， 该膜 在制备光转换发光膜时作为基材使用， 起到保护膜作用； 在使 用时能从光转化涂料层上很容易剥离下来。 由于采用氟素聚酯 膜作为基材， 在光转换发光膜制备时， 能起到涂布生产基材和 保护膜作用。 另外由于釆用的光转换涂料层主体树脂为有机硅 树脂， 树脂本身柔软带有弹性， 在剥离保护膜的时候容易发生 变形， 导致光转换膜厚度不均句， 从而影响发光性能， 因此本 发明釆用氟素聚酯膜作为基材和保护膜， 在使用时候可以很容 易将光转换涂料层从氟素聚酯膜上剥离下来， 避免了由于拉伸 引起的变形， 保证光转换膜的产品均勾， 稳定。
所述的氟素聚酯膜为表面涂覆氟素离型剂的聚脂膜。 其厚 度优选在 20 - Ι ΟΟμΐη,氟素聚酯膜在制备光转换发光膜时作为基 材使用， 在使用时能很容易从光转化涂料层上剥离下来， 使蓝 光光源直接照射在光转换发光膜上， 减少了光在氟素聚酯膜中 的折射， 提高了整体发光效率。
荧光材料为可以被蓝光激发的铝酸盐荧光材料、 硅酸盐荧 光材料、 硅氮化物荧光材料及硫氧化物荧光材料中的一种或两 种的组合； 荧光材料被做为激发光源的发射光镨在 440 ~ 475nm 范围内的蓝光 LED 激发， 吸收激发出至少一个以上峰值波长在 525 ~ 650nm 范围内的发射光谱; 荧光材料所发的光与蓝光 LED 所发的光复合成白色或其它颜色的光。
本发明所釆用的荧光材料需经过乙醇 -烷氧基低聚硅氧烷 混合液进行处理， 荧光材料经过混合液处理后， 可提高其与有 机硅树脂的相容性， 改善涂膜表面状态。
荧光材料的处理方法为热处理法， 具体步骤是在温度 80 - 90。C范围内， 将荧光材料与乙醇按比例投放入反应釜， 进行搅 拌， 然后再将烷氧基低聚硅氧烷投入反应釜中， 与粉体共同搅 拌， 最后将处理后粉体混合液进行抽滤， 干燥， 得到的荧光材 料即可在制备光转化涂料时直接使用。
本发明釆用的有机硅树脂为透明性好、 柔软、 弹性好的双 组分加成型加温硫化液体硅树脂。 这种树脂具有热氧化稳定性 好、 优异的电绝缘性能、 卓越的耐潮、 防水、 防锈、 耐寒、 耐 臭氧和耐候性能。 该树脂长时间在高温状态下工作也不会黄变， 并且固化后仍然柔韧性较好， 强度较高。 本发明釆用的有机硅 树脂优选粘度在 3000 -5000 cp. s , 透光率 >85%的硅树脂。
本发明涉及的可剥离型光转换发光膜的制备工艺为： 将荧 光材料先经过乙醇-烷氧基低聚硅氧烷混合液处理， 再将经混合 液处理后的荧光材料、 双组分有机硅树脂、 稀释剂和助剂按照 配比经研磨分散混合均勾， 再经过滤、 脱泡后， 涂布在氟素聚 酯膜表面， 经固化成型制得成品； 所述固化成型为热固化成型， 固化温度为： 150 ~ 200 。C。
稀释剂为曱苯、 二曱苯、 丁酯、 乙酯、 曱基硅油、 二曱基 硅油、 乙基硅油、 苯基硅油、 甲基苯基硅油中的一种或多种。
助剂可以采用紫外光吸收剂、 稳定剂、 流平剂、 消泡剂、 阻燃剂、 防沉剂、 润湿剂、 防静电剂中一种或多种。
本发明的有益效果：
1. 由于可剥离型光转换膜中的氟素聚酯膜在制备时作为 基材使用， 可以起到保护膜作用； 在使用时可以很容易剥离， 避免引起光转换涂料层的变形， 剥离后减少了光的折射， 提高 了发光效率。
2. 由于用来制备可剥离型光转换膜的荧光材料预先经过 乙醇-烷氧基低聚硅氧烷混合液， 因而提高了其与有机硅树脂的 相容性， 改善涂膜表面状态， 提高膜的均匀度。
3. 采用涂布法制备可剥离型光转换膜可以实现不同厚度 的涂布要求， 制备出各种厚度的光转换膜， 并且可以实现连续 生产， 生产效率高。 另外由于采用涂布方式对光转换涂料的粘 度和荧光材料的粒径要求比较宽， 更易于进行生产。 具体实施方式
实施例 1
荧光材料预处理： 将荧光材料与乙醇按比例 1 : 4投入在温 度 80。C的反应釜， 进行搅拌， 然后再将烷氧基低聚硅氧烷按荧 光材料 3%投入反应釜中， 与粉体共同搅拌 20min， 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料按以下配方 （质量百分 比） 配制成混合液：
双组分有机硅树脂 5
二曱苯 1
消泡剂 0. 1 流平剂 0. 1 铝酸盐荧光材料 2. 5 水 91. 3 上述原材料经研磨分散混合均勾， 再经过滤、 脱泡后， 涂 布在 20μπι氟素聚酯膜表面，经固化成型制得成品， 固化温度为： 150。C， 3min。 实施例 2
荧光材料预处理： 将荧光材料与乙醇按比例 1 : 3投入在温 度 90'C的反应釜， 进行搅拌， 然后再将垸氧基低聚硅氧烷按荧 光材料 4°/。投入反应釜中， 与粉体共同搅拌 30min， 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料经以下配方 （盾量百分 比） 配制成混合液：
双组分有机硅树脂 9 丁酯 0. 4 二甲苯 0. 6 消泡剂 0. 1 分散剂 0. 3 硅酸盐荧光材料 4. 2 水 85. 4 上述原材料经研磨分散混合均勾， 再经过滤、 脱泡后， 涂 布在 50μπι氟素聚酯膜表面，经固化成型制得成品， 固化温度为： 200°C, 2min。 实施例 3
荧光材料预处理： 将荧光材料与乙醇按比例 1 : 3投入在温 度 85。C的反应釜， 进行搅拌， 然后再将烷氧基低聚硅氧烷按荧 光材料 2%投入反应釜中， 与粉体共同搅拌 20min， 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料经以下配方 （质量百分 比） 配制成混合液：
双组分有机硅树脂 7
乙酯 0. 4 二曱苯 0. 4 消泡剂 0. 1 润湿剂 0. 2 分散剂 0. 4 硅氮化物荧光材料 4. 0 上述原材料经研磨分散混合均勾， 再经过滤、 脱泡后， 涂 布在 Ι ΟΟμπι 氟素聚酯膜表面， 经固化成型制得成品， 固化温度 为： 180°C, 2min。 实施例 4
荧光材 itt预处理： 将荧光材料与乙醇按比例 1 : 3投入在温 度 90。C的反应釜， 进行搅拌， 然后再将烷氧基低聚硅氧烷按荧 光材料 4%投入反应釜中， 与粉体共同搅拌 30min， 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料经以下配方 （质量百分 比） 配制成混合液：
双组分有机硅树脂 5
曱基娃油 0. 5
二曱基硅油 0. 5
消泡剂 0. 1
防沉剂 0. 1
硫氧化物荧光材料 2. 0
水 91. 8 上述原材料经研磨分散混合均勾， 再经过滤、 脱泡后， 涂 布在 75μΐη氟素聚酯膜表面，经固化成型制得成品， 固化温度为： 200°C, 1· 5min。 实施例 5
荧光材料预处理： 将发光材料与乙醇按比例 1 : 4投入在温 度 80。C的反应釜， 进行搅拌， 然后再将烷氧基低聚硅氧烷按发 光材料 3%投入反应釜中， 与粉体共同搅拌 20min， 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料经以下配方 （质量百 比） 配制成混合液：
双组分有机硅树脂 5
乙基硅油 1
消泡剂 0. 1
流平剂 0. 1
铝酸盐荧光材料 ' 2. 5
水 91. 3 上述原材料经研磨分散混合均勾， 再经过滤、 脱泡后， 涂 布在 20μΐη氟素聚酯膜表面，经固化成型制得成品， 固化温度为： 150°C, 3min。 实施例 6
荧光材料预处理： 将荧光材料与乙醇按比例 1 : 3投入在温 度 90°C的反应釜， 进行搅拌， 然后再将烷氧基低聚硅氧烷按发 光材料 4%投入反应釜中， 与粉体共同搅拌 30min, 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料经以下配方 （质量百分 比） 配制成混合液：
双组分有机硅树脂
苯基硅油
甲基苯基硅油
消泡剂
分散剂
硅氮化物荧光材料 水 85. 4 上述原材料经研磨分散混合均勾， 再经过滤、 脱泡后， 涂 布在 50μΐη氟素聚酯膜表面，经固化成型制得成品， 固化温度为： 200°C, 2min。 实施例 7
荧光材料预处理： 将荧光材料与乙醇按比例 1 : 3投入在温 度 90。C的反应釜， 进行搅拌， 然后再将烷氧基低聚硅氧烷按荧 光材料 4%投入反应釜中， 与粉体共同搅拌 30min， 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料经以下配方 （质量百分 比） 配制成混合液：
双组分有机硅树月
乙酯
甲苯
消泡剂
防沉剂
铝酸盐荧光材料
水
上述原材料经研磨分散混合均句， 再经过滤、 脱泡后， 涂 布在 75μΐη氟素聚酯膜表面，经固化成型制得成品， 固化温度为： 200°C, 1. 5min。 实施例 8
荧光材料预处理： 将荧光材料与乙醇按比例 1 : 3投入在温 度 85。C的反应釜， 进行搅拌， 然后再将烷氧基低聚硅氧烷按荧 光材料 2%投入反应釜中， 与粉体共同搅拌 20min， 将处理后粉 体液进行抽滤， 干燥得到处理好的荧光材料待用。
将处理好的荧光材料与其它原材料经以下配方 （质量百分 比） 配制成混合液：
双组分有机硅树脂 7
丁酯 0. 4
甲苯 0. 2
消泡剂 0. 1
润湿剂 0. 2
分散剂 0. 4
铝酸盐荧光材料 4. 0 水 87. 7 上述原材料经研磨分散混合均勾， 再经过滤、 脱泡后， 涂 布在 Ι ΟΟμπι 氟素聚酯膜表面， 经固化成型制得成品， 固化温度 为： 180。C, 2min。

Claims

权 利 要 求
1. 一种可剥离型光转换发光膜， 由基材和在其上的光转化 涂料层构成， 光转化涂料层由荧光材料、 双组分有机硅树脂、 稀 释剂和助剂组成，其特征在于所述的基材为氟素聚酯膜，在使用 光转换膜时氟素聚酯膜易于从光转化涂料层上剥离下来。
2. 根据权利要求 1所述的可剥离型光转换发光膜，其特征在 于所述的氟素聚酯膜为表面涂覆氟素离型剂的聚脂膜。
3. 根据权利要求 1 所述的可剥离型光转换发光膜， 其特征 在于所述的氟素聚酯膜总厚度为 20 - 100 μΐη。
4. 根据权利要求 1 所述的可剥离型光转换发光膜， 其特征 在于所述的荧光材料为可以被蓝光激发的铝酸盐荧光材料、硅酸 盐荧光材料、 硅氮化物荧光材料及硫氧化物荧光材料中的一种 或两种； 荧光材料被做为激发光源的发射光谱峰值波长在 440 ~ 475nm 范围内的蓝光 LED 激发， 发出至少一个以上峰值波长在 525 ~ 650nm 范围内的发射光谱； 荧光材料所发的光与蓝光 LED 所发的光复合成白色或其它颜色的光。
5. 根据权利要求 1 所述的可剥离型光转换发光膜， 其特征 在于所述的荧光材料需经过乙醇-烷氧基低聚硅氧烷混合液进 行处理。
6. 根据权利要求 1 所述的可剥离型光转换发光膜， 其特征 在于所述的稀释剂为甲苯、 二甲苯、 丁酯、 乙酯、 曱基硅油 V二 曱基硅油、 乙基硅油、苯基硅油、 甲基苯基硅油中的一种或多种。
7. 根据权利要求 1所述的可剥离型光转换发光膜， 其特征在 于助剂为紫外光吸收剂、 稳定剂、 流平剂、 消泡剂、 阻燃剂、 防 沉剂、 润湿剂、 防静电剂中一种或多种。
8. 制备如权利要求 1-7任一项所述的可剥离型光转换发光膜 的方法， 其包括步骤：
用乙醇-烷氧基低聚硅氧烷混合液处理荧光材料；
将经混合液处理后的荧光材料、 双组分有机硅树脂、 稀释剂 和助剂按照配比经研磨分散混合均匀， 并进行过滤、 脱泡， 得到 荧光材料分散液； 和
将荧光材料分散液涂布在氟素聚酯膜表面， 经固化成型制得 成品， 其中所述固化成型为热固化成型， 固化温度为： 150 ~
200 °C.
9. 根据权利要求 8所述的方法,其特征在于所述的氟素聚酯 膜为表面涂覆氟素离型剂的聚脂膜。
10. 根据权利要求 8 所述的方法， 其特征在于所述的氟素聚 酯膜总厚度为 20 - 100 μΐη。
11. 根据权利要求 8所述的方法，其特征在于所述的稀释剂为 甲苯、 二曱苯、 丁酯、 乙酯、 甲基硅油、 二曱基硅油、 乙基硅油、 苯基硅油、 曱基苯基硅油中的一种或多种。
12. 根据权利要求 8所述的方法，其特征在于所述助剂为紫外 光吸收剂、 稳定剂、 流平剂、 消泡剂、 阻燃剂、 防沉剂、 润湿剂、 防静电剂中一种或多种。
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